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Continuous polyamidation process - i

a polyamide and process technology, applied in the direction of chemical/physical/physical-chemical processes, liquid-liquid reaction processes, chemical apparatus and processes, etc., can solve the problems of reactor complexity and process scale-up complexity, chemical degradation of products, and increase in viscosity and gel build-up, so as to improve reactor size and output, simplify reactor design, and facilitate process scale-up and design

Active Publication Date: 2016-10-06
INV NYLON POLYMERS AMERICAS LLC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

The invention simplifies the design and operation of reactors, allows for larger reactors to be built, and increases output while reducing energy requirements and costs. It also improves the heat transfer and reduces sensitivity to materials in the reactor. The technical effects of the invention allow for larger and more efficient production of polyamide.

Problems solved by technology

However, the post-evaporation pressure reduction step requires excessive heat to prevent the product from solidifying, and this heating is known to cause discoloration and chemical degradation of the product.
However, the high temperatures required to retain the component(s) in melt form can result in degradation, and a number of methods (see, for instance, U.S. Pat. No. 4,131,712, U.S. Pat. No. 4,433,146 and U.S. Pat. No. 4,438,257) have sought to reduce such degradation and overcome associated difficulties.
Gel build-up occurs because, without direct means for controlling the chemical equilibria in the melt, the temperature rises due to the heat emitted by the polyamidation reaction which in turn causes evaporation of water produced by the polyamidation reaction thus causing a rise in viscosity and gel build-up.
However, there are several disadvantages associated with the use of mechanical agitation, including reactor complexity and complexity in process scale-up.
Agitators used in vertical multistage polyamidation reactors are complicated and expensive to design and manufacture as they require adequate mechanical strength to sufficiently agitate molten polyamide, but minimal surface area and roughness in order to limit the extent to which their surface provides nuclei for gelation.
However, as the size of the agitator is increased to cope with the increased size of the reactor, it becomes increasingly difficult to transmit the torque generated by the agitator across the diameter of the column.
Moreover, as the size of the mechanical agitator increases, its mechanical strength must also increase, which leads to difficulties in the design, fabrication and reliability of the component, as well as increased capital expenditure.
The effective limit on the size of the mechanical agitator in turn limits the size of the polyamidation reactor, and hence the production output.
In addition, processes and apparatus using conventional mechanical agitation are sensitive to perturbations of material in the reactor, and can suffer from poor reliability.

Method used

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  • Continuous polyamidation process - i
  • Continuous polyamidation process - i
  • Continuous polyamidation process - i

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0084]Adipic acid (AA) and hexamethylene diamine (HMD) are fed into a mixing tank at 162 lb / hr and 38 lb / hr, respectively. The heated mixture is fed into the top of an eight-stage reactor column at a rate of 199 lb / hr. Gaseous HMD is fed into the lowest three stages of the reactor at a rate of 90 lb / hr. During the reaction process, a stream C of steam is fed from a pressurised plenum at a rate of up to 20 lb / hr into a conical chamber below the lowest stage at the bottom of the reactor, the conical chamber being the region below the lowest stage in which is accumulated liquid phase material P rich in high molecular weight polyamide. The reactor is not equipped with an agitator, but otherwise comprises the features described in FIGS. 3a to 3d.

[0085]During operation of the reactor according to the invention, gaseous steam exits from the top of the reactor at a rate of 40 lb / hr without additional steam from stream C, or 60 lb / hr with additional steam from stream C, wherein the vapour e...

example 3

Column with Steam Sparging Made at 15.5 Inch Internal Diameter

[0093]A unit is designed for a nominal polymer production rate of 250 pounds per hour. A ten stage column is designed having 15.5 inch internal diameter for the top nine stages. The lowest stage smoothly reduces diameter in the head space down to a liquid inventory section having a constant internal diameter of 12 inches and a working depth of 24 inches (similar to that shown in FIG. 3g). The top nine stages are fitted with weirs to regulate the liquid inventory on each stage such that the hold-up time on each stage averages about 15 minutes. The inventory on the lowest stage is regulated by controlling the speed of the outlet pump.

[0094]This unit is fitted with temperature regulating jackets and coils identical to those of example 1. The temperature of the melt is again controlled.to reach 275° C. in the lowest stage.

[0095]The column is fitted with an agitator on the lowest stage, designed to turn at between 15 and 50 rp...

example 4

Column with Steam Sparging Made at 15.5 Inch Internal Diameter

[0099]A unit is designed for a nominal polymer production rate of 250 pounds per hour. A ten stage column is designed having 15.5 inch internal diameter for the top nine stages. The lowest stage is described by FIG. 3f with an unsparged but agitated conical section within a surrounding sparged melt pool. As shown in FIG. 3f, the lowest stage is also fitted with a plenum enabling the introduction of vapour through the melt pool. The top nine stages are fitted with weirs to regulate the liquid inventory on each stage such that the hold-up time on each stage averages about 15 minutes. The inventory on the lowest stage is regulated by controlling the speed of the outlet pump.

[0100]This unit is fitted with temperature regulating jackets and coils identical to those of example 1. The temperature of the melt is again controlled.to reach 275° C. in the lowest stage.

[0101]The column is fitted with an agitator only within the conic...

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Abstract

A continuous process for the manufacture of a polyamide, the process comprising the steps of: (i) flowing a stream A comprising a molten dicarboxylic acid, or a molten dicarboxylic acid-rich mixture comprising a dicarboxylic acid and a diamine, through a first stage and at least one more reaction stage of a vertical multistage reactor, wherein the first stage is at the top of the reactor; (ii) counter-currently flowing a stream B comprising a diamine as either a vapour or a diamine-rich liquid through at least one of the stages below the first reaction stage of said vertical multistage reactor; (iii) accumulating a liquid phase material P comprising polyamide at and / or below the final stage of said reactor; wherein said reactor is equipped with internal features suitable for effecting contact between counter-currently flowing streams A and B; and wherein said process further comprises the step of agitating said liquid phase material P by injecting a gaseous stream C comprising steam, or at least one inert gas, or a mixture of steam and at least one inert gas into the reactor at or below the final stage of the reactor. The invention further provides a vertical multistage reactor configured to implement said process.

Description

FIELD OF THE INVENTION[0001]The present invention relates to methods for the production of polyamides, and apparatus in which the polymerisation process can be conducted. More particularly, the present invention relates to continuous processes for the production of high molecular weight polyamides by the reaction of a dicarboxylic acid with a diamine via counter-current flow in a vertical multistage reactor.BACKGROUND OF THE INVENTION[0002]Polyamides, such as nylon-6,6, require starting monomers of two kinds, a monomer having a pair of carboxylic acid functional reactive groups (diacid) and a monomer having a pair of amino functional reactive groups (diamine), and such polyamides are typically referred to as dimonomeric polyamides. The polyamide may further incorporate more than one diacid and more than one diamine and may incorporate a small amount, usually no more than 10%, of a third kind of starting material having a carboxylic acid functional group and an amino functional group...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): C08G69/28
CPCC08G69/28B01J14/00B01J10/002B01J19/0006B01J19/006B01J19/0066B01J19/18B01J19/245B01J4/002B01J2219/00186B01J2219/002B01J2219/00202B01J2219/00231B29B7/826B29B7/002C08G69/26C08L77/00
Inventor MARCHILDON, ERNEST KEITHSURGENOR, KAREN A.KAUSHIVA, BRYAN D.
Owner INV NYLON POLYMERS AMERICAS LLC
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